CN105623202B - A kind of silicon nitride of high abrasion/polyester terephthalate nanocomposite and preparation method thereof - Google Patents

A kind of silicon nitride of high abrasion/polyester terephthalate nanocomposite and preparation method thereof Download PDF

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CN105623202B
CN105623202B CN201410669848.3A CN201410669848A CN105623202B CN 105623202 B CN105623202 B CN 105623202B CN 201410669848 A CN201410669848 A CN 201410669848A CN 105623202 B CN105623202 B CN 105623202B
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silicon nitride
polyester terephthalate
temperature
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abrasion
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CN105623202A (en
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杨桂生
苏荣锦
吕励耘
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Hefei Genius New Materials Co Ltd
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Abstract

It the present invention relates to a kind of high abrasion silicon nitride/polyester terephthalate nanocomposite and preparation method thereof, is made by passing through double screw extruder melting extrusion granulation after 95-99 parts of polyester terephthalates, 1-5 parts of modified nano silicon nitride particles, 0.5-3 parts of lubricants, the 0.1-1 parts of agitated mixing of antioxidant.Graininess is prepared after carrying out surface compound treatment to nano-silicon nitride with ethyl orthosilicate and coupling agent, improve dispersibility of the modified nano silicon nitride particle as anti-wear agent in matrix resin, so as to improve the caking property of anti-wear agent and polyester terephthalate matrix, high abrasion silicon nitride/polyester terephthalate nanocomposite obtained is set to increase significantly in terms of wear-resisting property, and maintain excellent mechanical property.

Description

A kind of silicon nitride of high abrasion/polyester terephthalate nanocomposite and its system Preparation Method
Technical field
The present invention relates to technical field of macromolecules, and in particular to a kind of silicon nitride/polyester terephthalate of high abrasion is received Nano composite material and preparation method thereof.
Background technique
With the development of technology, the polyester terephthalate class in thermoplastic polyester is on automobile using more and more extensive. Wherein being modified polybutylene terephthalate (PBT) (abbreviation PBT) plastics is most important car light material, it not only can reduce The quality of components about 40%, but also can make purchase cost reduce by 40% or so, therefore its dosage in the car it is rapid on It rises.In addition, PBT has good comprehensive performance, such as high-fire resistance, toughness, fatigue durability, self-lubricating, low-friction coefficient are weather-proof Property, water absorption rate are low etc..But the volume resistance of PBT is big, dielectric loss is big, and notch impact strength is low, and molding shrinkage is big.And gather Ethylene glycol terephthalate (abbreviation PET) is the polymer of highly crystalline, and smooth surface is glossy, in wider temperature model There is excellent physical mechanical property, for long-term use temperature up to 120 DEG C, electrical insulating property is excellent, or even in high-temperature high-frequency in enclosing Under, electrical property is still preferable, but corona resistance is poor, creep resistance, fatigue durability, and rub resistance, dimensional stability are all fine.
So meeting final component and customer demand in order to promote material property and class and generally passing through enhancing, filling, be total to The methods of mixed its processability of improvement and modification, it is obvious with glass fiber-reinforcing effect, resin rigidity, heat resistance, drug resistance can be improved Moral character, electric property and weatherability.But it still needs to improve the slow disadvantage of crystallization rate, the agent of addition type core and crystallization can be taken to promote The means such as agent.And in terms of wear-resisting modification, the common used material currently used for the wear-resisting modification of PBT, PET mainly has graphite, curing Molybdenum and polytetrafluoroethylene (PTFE), but the additive amount of these three materials is generally bigger, can come to polyester terephthalate material strips Defect: one will lead to the viscosity of composite material and density is larger;Second is that will affect the viscous of abrasion resistance modifier and PBT or PET matrix Knot property;Third is that the mechanical performance to composite material also has a significant impact, it is unfavorable for its application.
Summary of the invention
The object of the present invention is to provide a kind of high abrasion silicon nitride/polyester terephthalate nanocomposite and its preparations Method.
In order to achieve the object of the present invention, the present invention provides a kind of high abrasion silicon nitride/polyester terephthalate nanometers Composite material is prepared by weight by following components:
95-99 parts of polyester terephthalate
1-5 parts of modified nano silicon nitride particle
0.5-3 parts of lubricant
0.1-1 parts of antioxidant
The modified nano silicon nitride particle refers to nano-silicon nitride through ethyl orthosilicate and coupling agent compound base amount method The graininess that reconstruction grain is 2-5mm at partial size afterwards.
Preferably, the lubricant is silicone powder.
The antioxidant is four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant And the mixture of (2, the 4- di-tert-butyl-phenyl) ester of phosphorous acid three (irgasfos 168) 1010).
The coupling agent is gamma-aminopropyl-triethoxy-silane or γ-(methacryloxypropyl) propyl trimethoxy silicane.
The polyester terephthalate is polyethylene terephthalate (PET) or polybutylene terephthalate (PBT) (PBT).
It is a further object to provide above-mentioned high abrasion silicon nitride/polyester terephthalate nanocomposites Preparation method, including the following steps:
(1) nano-silicon nitride is added to and is in mass ratio by ammonium hydroxide and ethyl orthosilicate in mixed solution that 2:1 is formed, It is reacted 5-8 hours at 50-80 DEG C, obtains mixed liquor;
(2) coupling agent for accounting for nano-silicon nitride quality 0.5%-1.5% is added dropwise in mixed liquor in (1), it is anti-at 70-80 DEG C It answers 2-5 hours, deionized water rinsing, drying is used after centrifuge separation, it is 2- that granularity, which is made, finally by dry method rolling Granulation Equipments The modified nano silicon nitride particle of 5mm;
(3) by the modified nano silicon nitride handled through (2), antioxidant, lubricant and through what is be dried it is poly- to benzene two Formic acid esters is poured into high-speed mixer and is stirred, and is added twin-screw extrude after mixing, is granulated after melting extrusion, is made High abrasion silicon nitride/polyester terephthalate nanocomposite.
Further, one area's temperature of double screw extruder is 200-230 DEG C, and two area's temperature are 200-230 DEG C, three area's temperature Degree is 200-240 DEG C, and four area's temperature are 210-240 DEG C, and five area's temperature are 210-250 DEG C, and six area's temperature are 220-250 DEG C;It is double Screw host revolving speed is 250-500rpm.
The drying process of the polyester terephthalate is the dry 4-8h at 100-140 DEG C.
Beneficial effects of the present invention:
1, ethyl orthosilicate and coupling agent of the invention carry out surface compound treatment to nano-silicon nitride, improve as resistance to Dispersibility of the modified nano silicon nitride of grinding agent in matrix resin, so as to improve anti-wear agent and polyester terephthalate matrix Caking property, have high abrasion silicon nitride/polyester terephthalate nanocomposite obtained in terms of wear-resisting property significantly Raising, and maintain excellent mechanical property.
2, the modified nano silicon nitride particle used Jing Guo surface compound treatment of the invention is as anti-wear agent, than existing The additive amounts such as anti-wear agent graphite, molybdenum disulfide, polytetrafluoroethylene (PTFE) are few, and its density is small, mitigate while reducing production cost The weight of composite material expands its application range.
3, nano-silicon nitride is pressed into compact grain again after ethyl orthosilicate and coupling agent are composite modified by the present invention, from And its bulk density is increased, be conducive to the feeding of composite material extrusion process, further change while improving processing performance Dispersibility of the nano-silicon nitride in resin matrix has been apt to it, to improve the wearability of composite material.
4, nano silicon nitride silicon particle of the present invention also plays the effect of heterogeneous nucleation while serving as anti-wear agent, facilitates The slow disadvantage of polyester terephthalate crystallization rate is solved, improves the rigidity of product, heat distortion temperature, dimensional stability and transparent Degree and surface gloss.
Specific embodiment
The following describes the present invention further through the description of specific embodiments, but it is to limit of the invention that this, which is not, System, those skilled in the art's basic thought according to the present invention can make various modifications or improvements, but without departing from this The basic thought of invention, is all within the scope of the present invention.
Embodiment 1
(1) surface treating nano silicon nitride: it is 2:1 that nano-silicon nitride is added by ammonium hydroxide and ethyl orthosilicate in mass ratio In the mixed solution of composition, is reacted 6 hours at 60 DEG C, obtain mixed liquor;It is added dropwise in aforementioned mixed liquor again and accounts for nano silicon nitride The coupling agent gamma-aminopropyl-triethoxy-silane of siliceous amount 0.5% reacts 2 hours at 70 DEG C, deionization is used after centrifuge separation It is dried to obtain the modified nano silicon nitride of ethyl orthosilicate and coupling agent compound base amount method after water repeated flushing, is then led to It crosses dry method rolling Granulation Equipments and granularity is made in the modified nano silicon nitride particle of 2-5mm;
(2) drying process of PBT: dry 6h at a temperature of PBT is placed in 120 DEG C;
(3) silicon nitride/polyester terephthalate nanocomposite: the modified Nano that will be surface-treated through (1) is prepared 97 parts of PBT and 0.2 part of antioxidant 1010s, the 0.3 part of irgasfos 168 and 0.5 3 parts of silicon nitride particle and be dried through (2) Part lubricant silicone powder GM-100, which is poured into high-speed mixer, to be stirred, and is added twin-screw extrude after mixing, through melting High abrasion silicon nitride/polyester terephthalate nanocomposite is granulated to obtain after extrusion;
Wherein one area's temperature of double screw extruder is 200 DEG C, and two area's temperature are 210 DEG C, and three area's temperature are 220 DEG C, 4th area Temperature is 230 DEG C, and five area's temperature are 230 DEG C, and six area's temperature are 240 DEG C;Twin-screw engine speed is 350rpm.
Embodiment 2
(1) surface treating nano silicon nitride: it is 2:1 that nano-silicon nitride is added by ammonium hydroxide and ethyl orthosilicate in mass ratio In the mixed solution of composition, is reacted 8 hours at 50 DEG C, obtain mixed liquor;The coupling for accounting for nano-silicon nitride quality 1% is added dropwise again Agent gamma-aminopropyl-triethoxy-silane reacts 2 hours at 80 DEG C, with dry after deionized water repeated flushing after centrifuge separation The modified nano silicon nitride of ethyl orthosilicate and coupling agent compound base amount method is obtained, then sets it by dry method rolling granulation Granularity is prepared into the modified nano silicon nitride particle of 2-5mm;;
(2) drying process of PBT: dry 8h at a temperature of PBT is placed in 100 DEG C;
(3) silicon nitride/polyester terephthalate nanocomposite: the modified Nano that will be surface-treated through (1) is prepared 1 part of silicon nitride particle and 99 parts of PBT and 0.5 part of antioxidant 1010s, 0.5 part of irgasfos 168 and 1 part being dried through (2) Lubricant silicone powder GM-100, which is poured into high-speed mixer, to be stirred, and is added twin-screw extrude after mixing, is squeezed through melting High abrasion silicon nitride/polyester terephthalate nanocomposite is granulated to obtain after out;
Wherein one area's temperature of double screw extruder is 200 DEG C, and two area's temperature are 200 DEG C, and three area's temperature are 200 DEG C, 4th area Temperature is 210 DEG C, and five area's temperature are 210 DEG C, and six area's temperature are 220 DEG C;Twin-screw engine speed is 500rpm.
Embodiment 3
(1) surface treating nano silicon nitride: it is 2:1 that nano-silicon nitride is added by ammonium hydroxide and ethyl orthosilicate in mass ratio In the mixed solution of composition, is reacted 5 hours at 80 DEG C, obtain mixed liquor;The idol for accounting for nano-silicon nitride quality 1.5% is added dropwise again Join agent gamma-aminopropyl-triethoxy-silane, reacted 5 hours at 70 DEG C, is done after centrifuge separation with after deionized water repeated flushing Then it is granulated by the dry modified nano silicon nitride for obtaining ethyl orthosilicate and coupling agent compound base amount method by dry method rolling Granularity is made in the modified nano silicon nitride particle of 2-5mm in equipment;;
(2) drying process of PBT: dry 4h at a temperature of PBT is placed in 140 DEG C;
(3) silicon nitride/polyester terephthalate nanocomposite: the modified Nano that will be surface-treated through (1) is prepared 5 parts of silicon nitride particle and 95 parts of PET and 0.5 part of antioxidant 1010s, 0.3 part of irgasfos 168 and 3 parts being dried through (2) Lubricant silicone powder GM-100, which is poured into high-speed mixer, to be stirred, and is added twin-screw extrude after mixing, is squeezed through melting High abrasion silicon nitride/polyester terephthalate nanocomposite is granulated to obtain after out;
Wherein one area's temperature of double screw extruder is 220 DEG C, and two area's temperature are 230 DEG C, and three area's temperature are 235 DEG C, 4th area Temperature is 240 DEG C, and five area's temperature are 250 DEG C, and six area's temperature are 250 DEG C;Twin-screw engine speed is 250rpm.
Embodiment 4
(1) surface treating nano silicon nitride: it is 2:1 that nano-silicon nitride is added by ammonium hydroxide and ethyl orthosilicate in mass ratio In the mixed solution of composition, is reacted 6 hours at 60 DEG C, obtain mixed liquor;1% idol for accounting for nano-silicon nitride quality is added dropwise again Join agent γ-(methacryloxypropyl) propyl trimethoxy silicane, is reacted 4 hours at 75 DEG C, deionized water is used after centrifuge separation It is dried to obtain the modified nano silicon nitride of ethyl orthosilicate and coupling agent compound base amount method after repeated flushing, is then passed through Granularity is made in the modified nano silicon nitride particle of 2-5mm in dry method rolling Granulation Equipments;;
(2) drying process of PBT: dry 6h at a temperature of PBT is placed in 120 DEG C;
(3) silicon nitride/polyester terephthalate nanocomposite: the modified Nano that will be surface-treated through (1) is prepared 4 parts of silicon nitride particle be dried through (2) 96 parts of PET and 0.05 part of antioxidant 1010s, 0.05 part of irgasfos 168 and 0.5 part of lubricant silicone powder GM-100 is poured into high-speed mixer and is stirred, and is added twin-screw extrude after mixing, through molten High abrasion silicon nitride/polyester terephthalate nanocomposite is granulated to obtain after melting extrusion;
Wherein one area's temperature of double screw extruder is 230 DEG C, and two area's temperature are 230 DEG C, and three area's temperature are 240 DEG C, 4th area Temperature is 240 DEG C, and five area's temperature are 250 DEG C, and six area's temperature are 240 DEG C;Twin-screw engine speed is 250rpm.
Comparative example 1
(1) surface treating nano silicon nitride: it is 2:1 that nano-silicon nitride is added by ammonium hydroxide and ethyl orthosilicate in mass ratio In the mixed solution of composition, is reacted 6 hours at 60 DEG C, obtain mixed liquor;It is added dropwise in aforementioned mixed liquor again and accounts for nano silicon nitride The coupling agent gamma-aminopropyl-triethoxy-silane of siliceous amount 0.5% reacts 2 hours at 70 DEG C, deionization is used after centrifuge separation The modified nano silicon nitride powder of ethyl orthosilicate and coupling agent compound base amount method is dried to obtain after water repeated flushing;
(2) drying process of PBT: dry 6h at a temperature of PBT is placed in 120 DEG C;
(3) silicon nitride/polyester terephthalate nanocomposite: the modified Nano that will be surface-treated through (1) is prepared 97 parts of PBT and 0.2 part of antioxidant 1010s, the 0.3 part of irgasfos 168 and 0.5 they 3 parts of alpha-silicon nitride powders and be dried through (2) Part lubricant silicone powder GM-100, which is poured into high-speed mixer, to be stirred, and is added twin-screw extrude after mixing, through melting High abrasion silicon nitride/polyester terephthalate nanocomposite is granulated to obtain after extrusion;
Wherein one area's temperature of double screw extruder is 200 DEG C, and two area's temperature are 210 DEG C, and three area's temperature are 220 DEG C, 4th area Temperature is 230 DEG C, and five area's temperature are 230 DEG C, and six area's temperature are 240 DEG C;Twin-screw engine speed is 350rpm.
Comparative example 2
By 97 parts of PBT and 3 part of polytetrafluoroethylene powders of drying process, 0.2 part of antioxidant 1010,0.3 part of irgasfos 168 It pours into high-speed mixer and stirs with 0.5 part of lubricant silicone powder GM-100, add twin-screw extrude after mixing, pass through Polytetrafluoroethylene (PTFE)/PBT composite is granulated to obtain after melting extrusion;
Wherein one area's temperature of double screw extruder is 200 DEG C, and two area's temperature are 210 DEG C, and three area's temperature are 220 DEG C, 4th area Temperature is 230 DEG C, and five area's temperature are 230 DEG C, and six area's temperature are 240 DEG C;Twin-screw engine speed is 350rpm.
Comparative example 3
By 97 parts of PET and 3 part of polytetrafluoroethylene powders of drying process, 0.2 part of antioxidant 1010,0.3 part of irgasfos 168 It is poured into high-speed mixer with 0.5 part of lubricant silicone powder GM-100, high-speed stirred, mixes to uniformly rear and twin-screw extrusion is added In machine, polytetrafluoroethylene (PTFE)/PET composite material is granulated to obtain after melting extrusion;
Wherein one area's temperature of double screw extruder is 220 DEG C, and two area's temperature are 230 DEG C, and three area's temperature are 240 DEG C, 4th area Temperature is 240 DEG C, and five area's temperature are 250 DEG C, and six area's temperature are 250 DEG C;Twin-screw engine speed is 350rpm.
To the high abrasion silicon nitride/polyester terephthalate nanocomposite and comparative example 1 of above-described embodiment 1-4 preparation Polytetrafluoroethylene (PTFE)/PET composite material mechanical property of polytetrafluoroethylene (PTFE)/PBT composite and comparative example 2 preparation of preparation is adopted It is detected with ASTM standard, wear-resisting property is measured according to standard GB/T 5478-2008, and physical data is shown in Table 1.
1 performance data of table
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Comparative example 1 Comparative example 2 Comparative example 3
Tensile strength MPa 53 56 51 49 50 44 54
Notch impact strength KJ/m2 7.3 8.1 6.5 6.2 6.6 4.7 4.0
Wearability (750g, 1000r) 0.010 0.013 0.015 0.014 0.017 0.029 0.025
As shown in table 1, high abrasion silicon nitride/polyester terephthalate nanocomposite prepared by the present invention maintain compared with Good mechanical property, and very much, the wherein stretching of embodiment 2 is improved than the mechanical property of the composite material of comparative example 1-2 preparation Intensity and impact strength are best, respectively reach 56MPa, 8.1KJ/m2, improved respectively than comparative example nearly by 30%, 72%.Embodiment 1 with The comparison of comparative example 1 it is found that drying nano alpha-silicon nitride powders are pressed into after particle uses as anti-wear agent, the mechanical property of material with Wear-resisting property synergy is more preferable.In summary, it is 0.01-0.014 that the abrasion index of the product of preparation of the invention is extremely low, is showed Excellent wear-resisting property, composite material polyester terephthalate being modified with polytetrafluoroethylene (PTFE) than comparative example it is wear-resisting Performance wants excellent.Therefore, the anti-wear agent nano-silicon nitride obtained by the present invention significantly improves anti-wear agent and poly terephthalic acid The caking property of ester group body makes high abrasion silicon nitride/polyester terephthalate nanocomposite have anti-wear agent additive amount few, resistance to The advantages of mill protrudes, and mechanical property significantly improves.

Claims (8)

1. a kind of high abrasion silicon nitride/polyester terephthalate nanocomposite, it is characterised in that: by weight by following components Part is prepared:
95-99 parts of polyester terephthalate
1-5 parts of modified nano silicon nitride particle
0.5-3 parts of lubricant
0.1-1 parts of antioxidant
The modified nano silicon nitride particle refers to nano-silicon nitride after ethyl orthosilicate and coupling agent compound base amount method again The graininess that partial size is 2-5mm is made by dry method rolling Granulation Equipments.
2. high abrasion silicon nitride/polyester terephthalate nanocomposite according to claim 1, it is characterised in that: The lubricant is silicone powder.
3. high abrasion silicon nitride/polyester terephthalate nanocomposite according to claim 1, it is characterised in that: The antioxidant is four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters and phosphorous acid three (2,4- bis- Tert-butyl-phenyl) ester mixture.
4. high abrasion silicon nitride/polyester terephthalate nanocomposite according to claim 1, it is characterised in that: The coupling agent is gamma-aminopropyl-triethoxy-silane or γ-(methacryloxypropyl) propyl trimethoxy silicane.
5. high abrasion silicon nitride/polyester terephthalate nanocomposite according to claim 1, it is characterised in that: The polyester terephthalate is polyethylene terephthalate or polybutylene terephthalate (PBT).
6. a kind of prepare high abrasion silicon nitride as described in any one in claim 1-5/nano combined material of polyester terephthalate The method of material, it is characterised in that: include the following steps:
(1) nano-silicon nitride is added to and is in mass ratio by ammonium hydroxide and ethyl orthosilicate in mixed solution that 2:1 is formed, It is reacted 5-8 hours at 50-80 DEG C, obtains mixed liquor;
(2) coupling agent for accounting for nano-silicon nitride quality 0.5-1.5% is added dropwise in mixed liquor in (1), reacts 2-5 at 70-80 DEG C Hour, deionized water rinsing, drying is used after centrifuge separation, it is 2-5mm's that granularity, which is made, finally by dry method rolling Granulation Equipments Modified nano silicon nitride particle;
(3) by the modified nano silicon nitride handled through (2), antioxidant, lubricant and poly terephthalic acid through being dried Ester is poured into high-speed mixer and is stirred, and is added twin-screw extrude after mixing, is granulated after melting extrusion, is made high resistance to Grind silicon nitride/polyester terephthalate nanocomposite.
7. preparation method according to claim 6, it is characterised in that: one area's temperature of double screw extruder is 200- 230 DEG C, two area's temperature are 200-230 DEG C, and three area's temperature are 200-240 DEG C, and four area's temperature are 210-240 DEG C, and five area's temperature are 210-250 DEG C, six area's temperature are 220-250 DEG C;Twin-screw engine speed is 250-500rpm.
8. preparation method according to claim 6, it is characterised in that: the drying process of the polyester terephthalate be Dry 4-8h at 100-140 DEG C.
CN201410669848.3A 2014-11-21 2014-11-21 A kind of silicon nitride of high abrasion/polyester terephthalate nanocomposite and preparation method thereof Active CN105623202B (en)

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CN108929525A (en) * 2017-05-25 2018-12-04 合肥杰事杰新材料股份有限公司 A kind of polyethylene terephthalate composition and preparation method thereof
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CN87101054A (en) * 1987-05-29 1988-12-21 上海塑料厂 Anti-static and abrasion-resistant moulded bakelite
CN201208552Y (en) * 2008-05-07 2009-03-18 孙宝法 Dry process rolling granulator
CN103772973A (en) * 2014-01-06 2014-05-07 合肥杰事杰新材料股份有限公司 High-abrasion-resistance silicon nitride/nylon6 composite nano-material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN87101054A (en) * 1987-05-29 1988-12-21 上海塑料厂 Anti-static and abrasion-resistant moulded bakelite
CN201208552Y (en) * 2008-05-07 2009-03-18 孙宝法 Dry process rolling granulator
CN103772973A (en) * 2014-01-06 2014-05-07 合肥杰事杰新材料股份有限公司 High-abrasion-resistance silicon nitride/nylon6 composite nano-material and preparation method thereof

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